Blue-black sulfur dye.



UNITED STATES PATENT r es IAUL JULIUS, or LUDWIGSHAFEN, GERMANY, Assrenon TO THE canteens ANILIN AND SODA FABRIK, or sAMErLAcE.

BLUE-BLACK SULFUR DYE.

SPECIFICATION forming part of Letters Patent No. 648,753, dated May 1, 1900;

'Appllcation filed February 6, 1900.

To (0Z4 10/1/0712 it may concern:

Be it known that 1, PAUL JULIUS, doctor of philosophy, asubject of the Em peror of Aus triad-lungary, residing at Ludwigshafen-onthe-Rhine, in the Kingdom of Bavaria and Empire of Germany, have invented t'ul Improvements in Blue-Black new anduse- Dyestufis, of

which the following is a specification. My invention relates to the manufacture of a blue-black coloring-matter which directly dyes unmordanted cotton.

can be obtained from a certain meta-phenylendiamin derivative by treating the same with sulfur and sodium sultid. The said meta-phenylenrliamin derivative results from the condensation of symmetrical dinitro-meta-dichlorbenzene with para-amido-salicylic acid in aqueous solution and in the presence of a body that will bind the hydrochloric acid formed during the reaction, such as sodium carbonate or acetate. In this way dinitrodi para hydroxy-diphenyl-meta-phenylendiamin-di-carboxylic acid is obtained, which, judging from the manner of its formation,

and this when treated in the manner to be described with sulfur and sodi n m sulIid yields the coloring-matter which I do sire to claim.

- The following example will serve to further illustrate the manner in which my invention may be carried into practical effect and my new coloring-matter obtained. by weight.

The parts are Serial No. 4,262. (No specimens.)

Production of a bliteblack coloring-matter from dinitro dc' -para h'ydrowy diphen g L' meta phenylcndiamin d1) carboacyl'z'c', acid- Prepare the required initial material by heating to boiling in a reflux apparatus a' mixturi;

- acid thus obtained with forty Olparts of s'ulfur, one hundred and twenty (120) parts of crystallized sodium sulfid, and five (5) parts of water in an iron vessel. Gradually heat the mixture to about 140 centigrade while stirring and maintain at this temperature until the melt has become quite dry. WVhen cool, powder it up. In this condition it'can be directly used for dyeing purposes, or it may be 7-5 dissolved in a little water and salted outwith common salt. In this case when dyeing it is necessary to add soda, common salt, and sodium sulfid to the dyeing-bath in order to obtain the best results.

My new coloring-matter is readily soluble in water, its aqueous solution being blue green. Acids added to the solution produce a brown precipitate, which is redissolved by alkalies with a blue-green color. It dyes un- 85 mordanted cotton a blue black which is exceedingly fast to the action. of soap, light, and acids. It is but little altered in fastness or shade by subsequent treatment with chromates, copper-salts, and the like.

Now what I claim is- The new coloring matter; which can be obtain ed from dinitro di para hydroxydiphenyl meta phenylendiamin-di-carboxy1ic acid, by treating the same with sulfur and 5 sodium sulfid,.whose solution i'n'water is of a blue-green color dyeing unmordanted cotton a blue black, which is not materially altered in shade or fastiness by treatment with chremy hand in the presenee of two suiisri fiing mates and. copper-salts, and in which soinwitnesses. tion a brown precipitate is-formed on the addition ofJiydroehlorie acid, the said pi'ecipi- PAUL JULIUS 5 sate redissolving in alkalies with a blue- Witnesses; green color, substantiafly as described. J AOOB ADRIAN,

In testimony WllOYGOf I have hereunto set ERNEST/F. EHRHARDT. 

